A high-performance liquid chromatography/fluorescence method using multiple wavelength shift for simultaneous quantification of different PAH compounds was developed. The new method was superior to the methods of DONG and GREENBERG [J. Liquid Chromatogr. 11, 1887-1905 (1988)] and WISE et al. [Polycyclic aromat. Hydrocarb. (in press)] with respect to sensitivity of detection of the majority of 15 PAH compounds, and in particular of naphthalene, acenaphthene, fluorene and benzo(b)fluoranthene. The method of validation analysis employed showed that the new method is in statistical balance meaning that no systematic errors, and only small unsystematic errors, could be demonstrated. Furthermore, the method had a good reproducibility and a high sensitivity.